CN105420520A - Extraction method for vanadium in vanadium slag - Google Patents

Extraction method for vanadium in vanadium slag Download PDF

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Publication number
CN105420520A
CN105420520A CN201511010018.0A CN201511010018A CN105420520A CN 105420520 A CN105420520 A CN 105420520A CN 201511010018 A CN201511010018 A CN 201511010018A CN 105420520 A CN105420520 A CN 105420520A
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vanadium
residue
sodium
vanadium slag
slag
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CN201511010018.0A
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Chinese (zh)
Inventor
刘立新
温超
秦志波
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Panzhihua Henghong Iron Pellets Co Ltd
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Panzhihua Henghong Iron Pellets Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/20—Obtaining niobium, tantalum or vanadium
    • C22B34/22—Obtaining vanadium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/001—Dry processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/04—Working-up slag
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention relates to the technical field of vanadium hydrometallurgy, in particular to an extraction method for vanadium in vanadium slag. The extraction method for the vanadium in the vanadium slag comprises the following steps that a, the vanadium slag and sodium carbonate are evenly mixed; b, the mixed materials of the vanadium slag and the sodium carbonate are put into the upper portion of a shaft furnace for drying preheating; c, the preheated mixed materials of the vanadium slag and the sodium carbonate are roasted in the middle-lower portion of the shaft furnace, and oxygen is blasted toward the side face of the furnace bottom of the shaft furnace during the roasting process; d, the roasted materials are put into a wet grinder to be ground, and industrial water is added; e, the mixture of sodium vanadate and residues is obtained through grinding and filtered in a vacuum filter to obtain a sodium vanadate solution and the residues; and f, ammonium sulfate precipitation is added into the odium vanadate solution to obtain ammonium vanadate and a solution containing sodium salt, ammonium vanadate is separated out and subjected to dehydration and piece melting, and V2O5 is obtained. According to the extraction method for the vanadium in the vanadium slag, the production efficiency is improved.

Description

A kind of extracting method for Vanadium in Vanadium Residue
Technical field
The present invention relates to vanadium technical field of wet metallurgy, especially a kind of extracting method for Vanadium in Vanadium Residue.
Background technology
Vanadium slag refers to that the molten iron containing vanadium is oxidized into through the method such as to bessemerize and is rich in barium oxide (V 2o 3) a kind of slag, so in steel industry, vanadium slag is the main raw of vanadium extraction, from vanadium slag, extract vanadium is by the V of trivalent 2o 3change into the V of pentavalent 2o 5.At present, the extracting method of Vanadium in Vanadium Residue is vanadium slag sodium roasting-water logging, and the principle of vanadium slag sodium roasting-water logging is take vanadium slag as raw material, sodium carbonate as redox agent, by high-temperature roasting by the V in vanadium slag 2o 3being converted into vanadic acid sodium, is that the trivalent vanadium in vanadium slag is converted into pentavalent vanadium, and then add service water leaching and obtain sodium vanadate solution, add ammonium sulfate precipitation in the solution, obtain ammonium vanadate, ammonium vanadate obtains V through dehydration fuse piece 2o 5product.The equipment of vanadium slag sintering is generally multiple hearth furnace or rotary kiln, when adopting above-mentioned two kinds of roasting apparatus vanadium slag sinterings, Problems existing mainly contains the following aspects: (1) has higher oxidation ratio for making vanadium slag, usual employing improves the measure of temperature, easily causes materials from bonding on the inwall of equipment; (2) if avoid the generation of adhesion problem, the mode extending roasting time need be adopted to ensure that the transformation efficiency of vanadium touches the mark, cause production efficiency to reduce; (3), when adopting above-mentioned two kinds of equipment to carry out roasting, material and equipment inner wall rub, and to produce large dust more, and the leaching yield of vanadium can be caused to reduce, and to bring environment protection unfavorable simultaneously.
Summary of the invention
Technical problem to be solved by this invention is: the extracting method providing a kind of Vanadium in Vanadium Residue for enhancing productivity.
For solving the problems of the technologies described above the technical solution adopted in the present invention be: a kind of extracting method for Vanadium in Vanadium Residue, is characterized in that: comprise the steps:
A, by vanadium slag and sodium carbonate two kinds of material Homogeneous phase mixing;
B, vanadium slag and sodium carbonate mixture material are put into shaft furnace top carry out drying and forewarm;
C, the vanadium slag after preheating and sodium carbonate mixture material are carried out roasting in the middle and lower part of shaft furnace, in roasting process, advertise oxygen by vertical furnace bottom side regulate oxygen concentration in shaft furnace;
D, the material after step c roasting is put into wet wheeling machine grind, and add service water;
E, ground after, obtain vanadic acid sodium and residue mixture, molten for vanadic acid sodium and residue mixture are filtered in vacuum filter, obtain sodium vanadate solution and residue, if the vanadic acid sodium content in the residue after filtering is greater than 0.35%, then residue circulation is carried out steps d, until the vanadic acid sodium content in residue is less than 0.35%;
F, in sodium vanadate solution, add ammonium sulfate precipitation, obtain ammonium vanadate and containing sodium salt solution, separated by ammonium vanadate, ammonium vanadate obtains V through dehydration fuse piece 2o 5.
Further: V in described vanadium slag 2o 3content be 0.8 ~ 20% by mass percentage, vanadium slag is block or spherical.
Further: in step b, drying and forewarm temperature is 90 DEG C ~ 300 DEG C, and the drying and forewarm time is 0.5 ~ 2h.
Further: in step c, maturing temperature is 600 DEG C ~ 1000 DEG C, and roasting time is 1 ~ 3h.
Further: the oxygen concentration in step c in shaft furnace controls 40 ~ 80%.
Further: the content adding service water in steps d is 5 ~ 20% of vanadium slag and sodium carbonate mixture material gross weight.
Further: in steps d, wet-milling built-in temperature is 70 ~ 90 DEG C, the milling time of material is 0.5 ~ 2h.
The invention has the beneficial effects as follows: by shaft furnace, roasting is carried out to vanadium slag and sodium carbonate, oxygen is advertised to regulate the oxygen concentration in shaft furnace at vertical furnace bottom side in roasting process, ensure and improve the conversion rate of oxidation of vanadium slag, shortening the roasting oxidation time simultaneously, enhance productivity; During roasting, charging and discharging are carried out continuously, make stock column be in active state, and the bonding that effectively prevent material improves the conversion rate of oxidation of vanadium slag simultaneously, reduce the generation of dust; Material processing industry water grinding in wet wheeling machine is leached, and material fully grinds by wet wheeling machine, stir, and improves the leaching yield of vanadium.
Embodiment
For the ease of understanding the present invention, below in conjunction with embodiment, the present invention is further detailed.
A kind of extracting method for Vanadium in Vanadium Residue of the present invention carries out successively in accordance with the following steps:
A, by vanadium slag and sodium carbonate two kinds of material Homogeneous phase mixing, V in vanadium slag 2o 3content be by mass percentage 0.8 ~ 20% sodium carbonate as redox agent, the trivalent vanadium of vanadium slag is converted into pentavalent vanadium;
B, vanadium slag and sodium carbonate mixture material are put into shaft furnace top carry out drying and forewarm; Vanadium slag is block or spherical, and can reduce the generation of dust in roasting process, the temperature of shaft furnace inside exists steps difference, and the temperature on shaft furnace top controls between 90 DEG C ~ 300 DEG C, for carrying out drying and forewarm to vanadium slag and sodium carbonate mixture; Determine according to the vanadium slag added and sodium carbonate mixture weight, the drying and forewarm time is 0.5 ~ 2h;
C, the vanadium slag after preheating and sodium carbonate mixture are carried out roasting in the middle and lower part of shaft furnace, in roasting process, advertise oxygen by vertical furnace bottom side regulate oxygen concentration in shaft furnace, the both sides of shaft furnace are communicated with combustion chamber heating roasting material, maturing temperature is herein set to 600 DEG C ~ 1000 DEG C, roasting time is 1 ~ 3h, and the reaction of generation is 4FeO+4V 2o 3+ 4Na 2cO 3+ 5O 2=2Fe 2o 3+ 8NaVO 3+ 4CO 2; Side at the bottom of vertical furnace constantly blasts oxygen, ensures that the oxygen concentration in shaft furnace maintains 40 ~ 80%, ensures and improves the oxidation ratio of vanadium slag, shortening the time of roasting conversion simultaneously, enhance productivity; Meanwhile, because charging during roasting and discharging are carried out continuously, make stock column be in active state, effectively prevent the bonding of material, reduce the generation of dust;
D, the material after step c roasting is put into wet wheeling machine grind, and add service water, wet-milling built-in temperature controls between 70 ~ 90 DEG C, and the milling time of material is 0.5 ~ 2h; Service water plays the effect of dissolving, cooling, and the content adding service water is 5 ~ 20% of vanadium slag and sodium carbonate mixture material gross weight; Material fully grinds by wet wheeling machine, stir, and improve the leaching yield of vanadium, vanadic acid sodium enters liquid phase, and water-fast part is residue; In this step, service water can be lowered the temperature to vanadium slag and sodium carbonate mixture, the quality of grinding can be improved again, vanadic acid sodium can be made to be dissolved in service water to leach simultaneously, do not need the operation of separately material being lowered the temperature, reduce production cost, the heat simultaneously utilizing material to grind generation in wet wheeling machine ensures the leaching of vanadium, is enough used for heating service water or being incubated equipment;
E, ground after, obtain vanadic acid sodium and residue mixture, vanadic acid sodium and residue mixture are filtered in vacuum filter, obtain sodium vanadate solution and residue, if the vanadic acid sodium content in the residue after filtering is greater than 0.35%, then steps d is carried out in residue circulation, until the vanadic acid sodium content in residue is less than 0.35%, the raw material that residue can be used for blast furnace ironmaking uses;
F, in sodium vanadate solution, add ammonium sulfate precipitation, obtain ammonium vanadate and containing sodium salt solution, separated by ammonium vanadate, ammonium vanadate obtains V through dehydration fuse piece 2o 5.
In sum, by shaft furnace, roasting is carried out to vanadium slag and sodium carbonate, in roasting process, advertise oxygen to regulate the oxygen concentration in shaft furnace at vertical furnace bottom side, ensure and improve the oxidation ratio of vanadium slag, shortening the roasting oxidation time simultaneously, enhance productivity; During roasting, charging and discharging are carried out continuously, make stock column be in active state, effectively avoid the bonding of material; Material processing industry water grinding in wet wheeling machine is leached, and material fully grinds by wet wheeling machine, stir, and can improve the leaching yield of vanadium.
The result of following examples to be chemical composition diameter as shown in table 1 be 10 ~ 15mm vanadium slag gained under different technical parameters:
Table 1: the moiety of vanadium slag
V 2O 3 CaO SiO 2 MgO MnO FeO Ash content
Content/% 10.68 1.54 11.8 4.15 7.46 49.24 15.13
Embodiment 1:
By vanadium slag and sodium carbonate Homogeneous phase mixing, after adding shaft furnace, drying and forewarm temperature controls at 150 DEG C, drying time controls at 1h, maturing temperature controls at 600 DEG C, roasting time 2.5h, furnace bottom sidepiece amount of oxygen is 3 times that burning produces exhausted air quantity, roasting region oxygen concentration is about 79%, material tapping temperature is at about 100 DEG C, directly wet wheeling machine is entered after vanadium slag and sodium carbonate roasting, at wet wheeling machine material inlet, place adds normal temperature service water, control according to 6 tons/h, wet wheeling machine internal temperature is at about 80 DEG C, after material stops 1.8h in wet wheeling machine, discharging enters vacuum filter filtration, obtain sodium vanadate solution and residue, recording vanadic acid sodium content in residue is 0.55%, is returned in wet wheeling machine by residue and continues aforesaid operations, until vanadic acid sodium content is less than 0.35% in residue, then in sodium vanadate solution, add ammonium sulfate precipitation, obtain ammonium vanadate and contain sodium salt solution, ammonium vanadate obtains V through dehydration fuse piece 2o 5.
Embodiment 2:
By vanadium slag and sodium carbonate Homogeneous phase mixing, after adding shaft furnace, bake out temperature controls at 180 DEG C, drying time controls at 0.8h, maturing temperature controls at 850 DEG C, roasting time 2.0h, furnace bottom sidepiece amount of oxygen is 2 times that burning produces exhausted air quantity, roasting region oxygen concentration is about 73%, material tapping temperature is at about 140 DEG C, directly enter wet after vanadium slag and sodium carbonate roasting, at wet wheeling machine material inlet, place adds normal temperature service water, control according to 8.5 tons/h, wet wheeling machine internal temperature is at about 85 DEG C, after material stops 1.5h in wet wheeling machine, discharging enters vacuum filter filtration, obtain sodium vanadate solution and residue, recording vanadic acid sodium content in residue is 0.46%, is returned in wet wheeling machine by residue and continues aforesaid operations, until vanadic acid sodium content is less than 0.35% in residue, then in sodium vanadate solution, add ammonium sulfate precipitation, obtain ammonium vanadate and contain sodium salt solution, ammonium vanadate obtains V through dehydration fuse piece 2o 5.
Embodiment 3:
By vanadium slag and sodium carbonate Homogeneous phase mixing, after adding shaft furnace, bake out temperature controls at 200 DEG C, drying time controls at 0.6h, maturing temperature controls at 1000 DEG C, roasting time 1.5h, furnace bottom sidepiece amount of oxygen is 1.8 times that burning produces exhausted air quantity, roasting region oxygen concentration is about 70%, pelletizing tapping temperature is at about 160 DEG C, directly enter wet after vanadium slag and sodium carbonate roasting, at wet wheeling machine material inlet, place adds normal temperature service water, control according to 10 tons/h, wet wheeling machine internal temperature is at about 85 DEG C, after material stops 1.3h in wet wheeling machine, discharging enters vacuum filter filtration, obtain sodium vanadate solution and residue, recording vanadic acid sodium content in residue is 0.34%, then in sodium vanadate solution, ammonium sulfate precipitation is added, obtain ammonium vanadate and contain sodium salt solution, ammonium vanadate obtains V through dehydration fuse piece 2o 5.

Claims (7)

1. for an extracting method for Vanadium in Vanadium Residue, it is characterized in that: comprise the steps:
A, by vanadium slag and sodium carbonate two kinds of material Homogeneous phase mixing;
B, vanadium slag and sodium carbonate mixture material are put into shaft furnace top carry out drying and forewarm;
C, the vanadium slag after preheating and sodium carbonate mixture material are carried out roasting in the middle and lower part of shaft furnace, in roasting process, advertise oxygen by vertical furnace bottom side regulate oxygen concentration in shaft furnace;
D, the material after step c roasting is put into wet wheeling machine grind, and add service water;
E, ground after, obtain vanadic acid sodium and residue mixture, vanadic acid sodium and residue mixture are filtered in vacuum filter, obtain sodium vanadate solution and residue, if the vanadic acid sodium content in the residue after filtering is greater than 0.35%, then residue circulation is carried out steps d, until the vanadic acid sodium content in residue is less than 0.35%;
F, in sodium vanadate solution, add ammonium sulfate precipitation, obtain ammonium vanadate and containing sodium salt solution, separated by ammonium vanadate, ammonium vanadate obtains V through dehydration fuse piece 2o 5.
2. a kind of extracting method for Vanadium in Vanadium Residue as claimed in claim 1, is characterized in that: V in described vanadium slag 2o 3content be 0.8 ~ 20% by mass percentage, vanadium slag is block or spherical.
3. a kind of extracting method for Vanadium in Vanadium Residue as claimed in claim 1, is characterized in that: in step b, drying and forewarm temperature is 90 DEG C ~ 300 DEG C, and the drying and forewarm time is 0.5 ~ 2h.
4. a kind of extracting method for Vanadium in Vanadium Residue as claimed in claim 1, is characterized in that: in step c, maturing temperature is 600 DEG C ~ 1000 DEG C, and roasting time is 1 ~ 3h.
5. a kind of extracting method for Vanadium in Vanadium Residue as claimed in claim 1, is characterized in that: in step c, the oxygen concentration of shaft furnace middle and lower part controls 40 ~ 80%.
6. a kind of extracting method for Vanadium in Vanadium Residue as claimed in claim 1, is characterized in that: the content adding service water in steps d is 5 ~ 20% of vanadium slag and sodium carbonate mixture material gross weight.
7. a kind of extracting method for Vanadium in Vanadium Residue as claimed in claim 1, it is characterized in that: in steps d, wet-milling built-in temperature is 70 ~ 90 DEG C, the milling time of material is 0.5 ~ 2h.
CN201511010018.0A 2015-12-29 2015-12-29 Extraction method for vanadium in vanadium slag Pending CN105420520A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106145188A (en) * 2016-07-05 2016-11-23 河北钢铁股份有限公司承德分公司 A kind of method that sodium vanadium extraction liquid prepares V electrolyte high purity vanadic anhydride
CN106399665A (en) * 2016-10-21 2017-02-15 中钢集团鞍山热能研究院有限公司 Inferior coal vanadium extraction pure oxygen roasting method and device
CN107119191A (en) * 2017-06-30 2017-09-01 攀钢集团研究院有限公司 A kind of extracting method for Vanadium in Vanadium Residue
CN109234521A (en) * 2018-11-28 2019-01-18 承德燕北冶金材料有限公司 A method of the vanadium extraction again of the ferric vandate of byproduct containing vanadium
CN110106345A (en) * 2019-06-24 2019-08-09 攀钢集团研究院有限公司 Roasting clinker mechanical activation leching prepares method of the low sodium vanadium than leachate
CN112458298A (en) * 2020-10-27 2021-03-09 攀钢集团攀枝花钢铁研究院有限公司 Method for extracting vanadium by direct sodium treatment of thermal vanadium slag
CN114262799A (en) * 2021-12-28 2022-04-01 中国科学院过程工程研究所 Method for cleanly extracting vanadium from vanadium-containing steel slag
CN114350933A (en) * 2021-11-29 2022-04-15 攀钢集团研究院有限公司 Sodium removal method for vanadium extraction residue by sodium method

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106145188A (en) * 2016-07-05 2016-11-23 河北钢铁股份有限公司承德分公司 A kind of method that sodium vanadium extraction liquid prepares V electrolyte high purity vanadic anhydride
CN106399665A (en) * 2016-10-21 2017-02-15 中钢集团鞍山热能研究院有限公司 Inferior coal vanadium extraction pure oxygen roasting method and device
CN107119191A (en) * 2017-06-30 2017-09-01 攀钢集团研究院有限公司 A kind of extracting method for Vanadium in Vanadium Residue
CN107119191B (en) * 2017-06-30 2018-10-30 攀钢集团研究院有限公司 A kind of extracting method for Vanadium in Vanadium Residue
CN109234521A (en) * 2018-11-28 2019-01-18 承德燕北冶金材料有限公司 A method of the vanadium extraction again of the ferric vandate of byproduct containing vanadium
CN110106345A (en) * 2019-06-24 2019-08-09 攀钢集团研究院有限公司 Roasting clinker mechanical activation leching prepares method of the low sodium vanadium than leachate
CN112458298A (en) * 2020-10-27 2021-03-09 攀钢集团攀枝花钢铁研究院有限公司 Method for extracting vanadium by direct sodium treatment of thermal vanadium slag
CN114350933A (en) * 2021-11-29 2022-04-15 攀钢集团研究院有限公司 Sodium removal method for vanadium extraction residue by sodium method
CN114350933B (en) * 2021-11-29 2024-04-26 攀钢集团研究院有限公司 Sodium removal method for sodium-method vanadium extraction residues
CN114262799A (en) * 2021-12-28 2022-04-01 中国科学院过程工程研究所 Method for cleanly extracting vanadium from vanadium-containing steel slag

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